#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:01:06 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298095 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/30/1573036.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1573036
loop_
_publ_author_name
'Závodná, Aneta'
'Janovský, Petr'
'Kolařík, Václav'
'Ward, Jas S.'
'Prucková, Zdeňka'
'Rouchal, Michal'
'Rissanen, Kari'
'Vícha, Robert'
_publ_section_title
;
 Allosteric release of cucurbit[6]uril from a rotaxane using a molecular
 signal.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              83
_journal_page_last               89
_journal_paper_doi               10.1039/d4sc03970j
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety
'C36 H36 N24 O12, C22 H44 N2, 2(F6 P), 5.75(H2 O)'
_chemical_formula_sum            'C58 H91.5 F12 N26 O17.75 P2'
_chemical_formula_weight         1727.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-18 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.47878(10)
_cell_length_b                   27.72924(12)
_cell_length_c                   15.22975(7)
_cell_measurement_reflns_used    57423
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.4810
_cell_measurement_theta_min      3.1720
_cell_volume                     7381.45(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  41.00   0.50    0.40    --   46.00  91.00 -92.06   54
  2  ω   -119.00 -27.00   0.50    0.40    --  -51.89 -77.00-150.00  184
  3  ω     -4.00  25.00   0.50    0.40    --  -51.89  19.00-120.00   58
  4  ω     -4.00  25.00   0.50    0.40    --  -51.89  19.00   0.00   58
  5  ω     19.00 104.00   0.50    0.40    --   51.89-125.00   0.00  170
  6  ω   -129.00 -37.00   0.50    0.40    --  -62.00 -77.00 136.44  184
  7  ω   -148.00 -58.00   0.50    0.40    --  -78.00 -69.00  34.84  180
  8  ω   -155.00 -86.00   0.50    1.50    --  -87.58 -99.00 120.00  138
  9  ω   -112.00 -20.00   0.50    1.50    --  -87.58  77.00  90.00  184
 10  ω   -112.00 -20.00   0.50    1.50    --  -87.58  77.00-150.00  184
 11  ω    -54.00 -13.00   0.50    1.50    --  -87.58  57.00   0.00   82
 12  ω   -168.00 -77.00   0.50    1.50    --  -95.50 -62.00-174.58  182
 13  ω     88.00 176.00   0.50    1.50    --  102.12  38.00 120.00  176
 14  ω     80.00 173.00   0.50    1.50    --  102.12 125.00-120.00  186
 15  ω     25.00  52.00   0.50    1.50    --  102.12 -38.00-120.00   54
 16  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00-120.00  142
 17  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00 150.00  142
 18  ω     88.00 176.00   0.50    1.50    --  102.12  38.00 150.00  176
 19  ω     25.00  52.00   0.50    1.50    --  102.12 -38.00 -60.00   54
 20  ω     63.00 176.00   0.50    1.50    --  102.12  19.00  60.00  226
 21  ω     28.00  79.00   0.50    1.50    --  102.12 -57.00 150.00  102
 22  ω     32.00 111.00   0.50    1.50    --  102.12-125.00   0.00  158
 23  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00  90.00  142
 24  ω     32.00 111.00   0.50    1.50    --  102.12-125.00  30.00  158
 25  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00  30.00  142
 26  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00  60.00  142
 27  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00 -90.00  142
 28  ω     28.00  79.00   0.50    1.50    --  102.12 -57.00   0.00  102
 29  ω     32.00 111.00   0.50    1.50    --  102.12-125.00-120.00  158
 30  ω     25.00  52.00   0.50    1.50    --  102.12 -38.00-150.00   54
 31  ω     35.00 106.00   0.50    1.50    --  102.12 -99.00 -60.00  142
 32  ω     25.00  52.00   0.50    1.50    --  102.12 -38.00 150.00   54
 33  ω     28.00  79.00   0.50    1.50    --  102.12 -57.00 -90.00  102
 34  ω     28.00  79.00   0.50    1.50    --  102.12 -57.00-150.00  102
 35  ω     88.00 176.00   0.50    1.50    --  102.12  38.00  90.00  176
 36  ω     35.00 127.00   0.50    1.50    --  102.12 -77.00 150.00  184
 37  ω     88.00 176.00   0.50    1.50    --  102.12  38.00-150.00  176
 38  ω     14.00  41.00   0.50    0.40    --   46.00  91.00 -12.23   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0009372000
_diffrn_orient_matrix_UB_12      -0.0182524000
_diffrn_orient_matrix_UB_13      0.0955312000
_diffrn_orient_matrix_UB_21      -0.0881454000
_diffrn_orient_matrix_UB_22      0.0009593000
_diffrn_orient_matrix_UB_23      -0.0005575000
_diffrn_orient_matrix_UB_31      -0.0012609000
_diffrn_orient_matrix_UB_32      -0.0524575000
_diffrn_orient_matrix_UB_33      -0.0332202000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74539
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             3606
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/water'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 3643 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         7788
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0766P)²+4.5628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7679
_reflns_number_total             7788
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03970j2.cif
_cod_data_source_block           6b
_cod_depositor_comments
'Adding full bibliography for 1573035--1573038.cif.'
_cod_original_formula_sum        'C58 H91.50 F12 N26 O17.75 P2'
_cod_database_code               1573036
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.784
_diffrn_oxdiff_digest_frames
;
01de2715c855156fc377cccee391bee22105104eec3
;
_diffrn_oxdiff_digest_hkl
;
01659cb8d32a4ddcde798744813a382b6fe36a
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O231, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H27A,H27B} of O271, {H22C,H22D} of O221, {H21A,H21B}
  of O211, {H25A,H25B} of O251, {H28A,H28B} of O281, {H23A,H23B} of O231, {H24C,
  H24D} of O241, {H20C,H20D} of O201, {H26A,H26B} of O261
2. Restrained distances
 H20C-O211_$1
 1.97 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C3)
Uanis(O281) = Uanis(O261)
Uanis(O251) = Uanis(O271)
4. Rigid body (RIGU) restrains
5. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) N5(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) N12(0.5)
 H12A(0.5) H12B(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 C19(0.5) H19(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) C23(0.5) H23(0.5) C24(0.5) H24A(0.5) H24B(0.5) O201(0.5)
 H20C(0.5) H20D(0.5) O211(0.5) H21A(0.5) H21B(0.5) O221(0.25) H22C(0.25)
 H22D(0.25) O231(0.25) H5A(0.5) H5B(0.5) H23A(0.25) H23B(0.25) O241(0.5)
 H24C(0.5) H24D(0.5) O251(0.25) H25A(0.25) H25B(0.25) O261(0.25) H26A(0.25)
 H26B(0.25) O271(0.125) H27A(0.125) H27B(0.125) O281(0.25) H28A(0.25) H28B(0.25)
 Fixed X: H22C(0.46586) H22D(0.50364) H5A(0.25177) H5B(0.310881) H23A(0.4042)
 H23B(0.327361) H25A(0.667741) H25B(0.64345) H26A(0.54614) H26B(0.603741)
 H27A(0.504709) H27B(0.46098) H28A(0.599509) H28B(0.5303)
 Fixed Y: H22C(0.59084) H22D(0.60171) H5A(0.87596) H5B(0.86683) H23A(0.57038)
 H23B(0.556789) H25A(0.68209) H25B(0.64666) H26A(0.5402) H26B(0.55254)
 H27A(0.476159) H27B(0.515321) H28A(0.542729) H28B(0.55248)
 Fixed Z: H22C(0.39735) H22D(0.317141) H5A(0.87464) H5B(0.80297)
 H23A(0.409619) H23B(0.42699) H25A(0.55282) H25B(0.49599) H26A(0.509419)
 H26B(0.571321) H27A(0.40821) H27B(0.43188) H28A(0.617701) H28B(0.65696)
6.a Free rotating group:
 O201(H20C,H20D), O211(H21A,H21B), O241(H24C,H24D)
6.b Ternary CH refined with riding coordinates:
 C2(H2), C19(H19), C21(H21), C23(H23), C54(H54), C66(H66), C70(H70), C78(H78),
 C82(H82), C94(H94)
6.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), N12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B),
  C24(H24A,H24B), C61(H61A,H61B), C62(H62A,H62B), C73(H73A,H73B), C74(H74A,
 H74B), C85(H85A,H85B), C86(H86A,H86B)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.798
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2857(6) 0.9682(3) 0.9092(6) 0.063(2) Uani 0.5 1 d . . . A -1
H1A H 0.2591 0.9594 0.9635 0.095 Uiso 0.5 1 calc GR . . A -1
H1B H 0.2530 0.9608 0.8587 0.095 Uiso 0.5 1 calc GR . . A -1
H1C H 0.2975 1.0027 0.9099 0.095 Uiso 0.5 1 calc GR . . A -1
C2 C 0.3601(5) 0.9394(3) 0.9022(8) 0.0632(17) Uani 0.5 1 d . . . A -1
H2 H 0.3747 0.9414 0.8388 0.076 Uiso 0.5 1 calc R . . A -1
C3 C 0.4219(5) 0.9620(3) 0.9481(8) 0.0632(17) Uani 0.5 1 d . . . A -1
H3A H 0.4226 0.9966 0.9345 0.095 Uiso 0.5 1 calc GR . . A -1
H3B H 0.4704 0.9474 0.9298 0.095 Uiso 0.5 1 calc GR . . A -1
H3C H 0.4151 0.9576 1.0115 0.095 Uiso 0.5 1 calc GR . . A -1
C4 C 0.3512(11) 0.8831(6) 0.9212(8) 0.049(3) Uani 0.5 1 d . . . A -1
H4A H 0.4012 0.8668 0.9146 0.059 Uiso 0.5 1 calc R . . A -1
H4B H 0.3329 0.8779 0.9820 0.059 Uiso 0.5 1 calc R . . A -1
N5 N 0.2955(4) 0.86285(18) 0.8580(3) 0.0356(12) Uani 0.5 1 d . . . A -1
C6 C 0.2881(4) 0.8105(2) 0.8723(4) 0.0335(12) Uani 0.5 1 d . . . A -1
H6A H 0.2665 0.8049 0.9315 0.040 Uiso 0.5 1 calc R . . A -1
H6B H 0.3396 0.7957 0.8705 0.040 Uiso 0.5 1 calc R . . A -1
C7 C 0.2375(8) 0.7857(2) 0.8048(4) 0.034(4) Uani 0.5 1 d . . . A -1
H7A H 0.1890 0.8040 0.7999 0.040 Uiso 0.5 1 calc R . . A -1
H7B H 0.2249 0.7530 0.8265 0.040 Uiso 0.5 1 calc R . . A -1
C8 C 0.2727(3) 0.7811(2) 0.7134(4) 0.0317(13) Uani 0.5 1 d . . . A -1
H8A H 0.2718 0.8132 0.6846 0.038 Uiso 0.5 1 calc R . . A -1
H8B H 0.3268 0.7713 0.7195 0.038 Uiso 0.5 1 calc R . . A -1
C9 C 0.2320(3) 0.7452(2) 0.6546(4) 0.0313(17) Uani 0.5 1 d . . . A -1
H9A H 0.1770 0.7535 0.6518 0.038 Uiso 0.5 1 calc R . . A -1
H9B H 0.2366 0.7126 0.6805 0.038 Uiso 0.5 1 calc R . . A -1
C10 C 0.2648(5) 0.7446(2) 0.5622(4) 0.034(3) Uani 0.5 1 d . . . A -1
H10A H 0.3213 0.7431 0.5657 0.041 Uiso 0.5 1 calc R . . A -1
H10B H 0.2509 0.7751 0.5323 0.041 Uiso 0.5 1 calc R . . A -1
C11 C 0.2360(5) 0.70232(19) 0.5079(3) 0.029(3) Uani 0.5 1 d . . . A -1
H11A H 0.2657 0.6736 0.5261 0.035 Uiso 0.5 1 calc R . . A -1
H11B H 0.1822 0.6964 0.5254 0.035 Uiso 0.5 1 calc R . . A -1
N12 N 0.2378(12) 0.70409(17) 0.4157(3) 0.041(4) Uani 0.5 1 d . . . A -1
H12A H 0.2750 0.7255 0.4007 0.049 Uiso 0.5 1 calc R . . A -1
H12B H 0.1926 0.7172 0.3981 0.049 Uiso 0.5 1 calc R . . A -1
C13 C 0.2500 0.66119(15) 0.3625(3) 0.0375(10) Uani 1 2 d S T P . .
H13A H 0.2000 0.6446 0.3581 0.045 Uiso 0.5 1 calc R . . A -1
H13B H 0.2840 0.6397 0.3967 0.045 Uiso 0.5 1 calc R . . A -1
C14 C 0.2813(4) 0.6634(2) 0.2736(4) 0.0305(11) Uani 0.5 1 d . . . A -1
H14A H 0.3378 0.6613 0.2766 0.037 Uiso 0.5 1 calc R . . A -1
H14B H 0.2679 0.6948 0.2469 0.037 Uiso 0.5 1 calc R . . A -1
C15 C 0.2500 0.62097(15) 0.2122(3) 0.0445(11) Uani 1 2 d S TU P . .
C16 C 0.1763(4) 0.6202(2) 0.1876(4) 0.0368(13) Uani 0.5 1 d . U . A -1
H16A H 0.1631 0.6513 0.1596 0.044 Uiso 0.5 1 calc R . . A -1
H16B H 0.1436 0.6164 0.2403 0.044 Uiso 0.5 1 calc R . . A -1
C17 C 0.3090(4) 0.6278(2) 0.1267(4) 0.0377(13) Uani 0.5 1 d . U . A -1
H17A H 0.2994 0.6592 0.0977 0.045 Uiso 0.5 1 calc R . . A -1
H17B H 0.3629 0.6272 0.1469 0.045 Uiso 0.5 1 calc R . . A -1
C18 C 0.2834(5) 0.5721(2) 0.2528(5) 0.0466(17) Uani 0.5 1 d . U . A -1
H18A H 0.3390 0.5755 0.2635 0.056 Uiso 0.5 1 calc R . . A -1
H18B H 0.2580 0.5650 0.3095 0.056 Uiso 0.5 1 calc R . . A -1
C19 C 0.1595(5) 0.5791(3) 0.1233(5) 0.0486(17) Uani 0.5 1 d . U . A -1
H19 H 0.1039 0.5789 0.1077 0.058 Uiso 0.5 1 calc R . . A -1
C20 C 0.2081(12) 0.5883(8) 0.0407(13) 0.049(3) Uani 0.5 1 d . U . A -1
H20A H 0.1942 0.5644 -0.0049 0.059 Uiso 0.5 1 calc R . . A -1
H20B H 0.1963 0.6208 0.0174 0.059 Uiso 0.5 1 calc R . . A -1
C21 C 0.2938(12) 0.5847(8) 0.0594(13) 0.048(3) Uani 0.5 1 d . U . A -1
H21 H 0.3241 0.5893 0.0044 0.058 Uiso 0.5 1 calc R . . A -1
C22 C 0.3147(7) 0.5384(3) 0.1031(6) 0.063(2) Uani 0.5 1 d . U . A -1
H22A H 0.3700 0.5386 0.1172 0.076 Uiso 0.5 1 calc R . . A -1
H22B H 0.3049 0.5113 0.0622 0.076 Uiso 0.5 1 calc R . . A -1
C23 C 0.2687(7) 0.5305(2) 0.1876(5) 0.052(3) Uani 0.5 1 d . U . A -1
H23 H 0.2830 0.4990 0.2150 0.062 Uiso 0.5 1 calc R . . A -1
C24 C 0.1821(8) 0.5308(3) 0.1645(7) 0.061(3) Uani 0.5 1 d . U . A -1
H24A H 0.1708 0.5044 0.1228 0.074 Uiso 0.5 1 calc R . . A -1
H24B H 0.1516 0.5254 0.2184 0.074 Uiso 0.5 1 calc R . . A -1
C52 C 0.2500 0.90357(11) 0.6179(2) 0.0206(7) Uani 1 2 d S T P . .
N53 N 0.31336(13) 0.90404(8) 0.56514(14) 0.0243(4) Uani 1 1 d . . . . .
C54 C 0.29458(15) 0.90701(9) 0.47243(17) 0.0220(5) Uani 1 1 d . . . . .
H54 H 0.3158 0.9369 0.4449 0.026 Uiso 1 1 calc R . . . .
N55 N 0.31321(13) 0.86442(8) 0.42223(14) 0.0226(4) Uani 1 1 d . . . . .
C56 C 0.2500 0.84131(12) 0.3900(2) 0.0215(6) Uani 1 2 d S T P . .
O59 O 0.2500 0.90389(9) 0.69778(17) 0.0264(5) Uani 1 2 d S T P . .
O60 O 0.2500 0.80637(10) 0.34069(17) 0.0262(5) Uani 1 2 d S T P . .
C61 C 0.39012(16) 0.90694(10) 0.59973(18) 0.0254(5) Uani 1 1 d . . . . .
H61A H 0.3877 0.9180 0.6615 0.031 Uiso 1 1 calc R . . . .
H61B H 0.4191 0.9313 0.5659 0.031 Uiso 1 1 calc R . . . .
C62 C 0.38899(15) 0.85445(9) 0.38893(17) 0.0244(5) Uani 1 1 d . . . . .
H62A H 0.4148 0.8854 0.3761 0.029 Uiso 1 1 calc R . . . .
H62B H 0.3843 0.8365 0.3330 0.029 Uiso 1 1 calc R . . . .
N63 N 0.43129(13) 0.86119(8) 0.59646(15) 0.0250(5) Uani 1 1 d . . . . .
C64 C 0.45326(15) 0.83788(10) 0.67269(17) 0.0255(5) Uani 1 1 d . . . . .
N65 N 0.50510(14) 0.80293(9) 0.65048(15) 0.0261(5) Uani 1 1 d . . . . .
C66 C 0.52088(15) 0.80124(9) 0.55765(17) 0.0234(5) Uani 1 1 d . . . . .
H66 H 0.5770 0.8028 0.5453 0.028 Uiso 1 1 calc R . . . .
N67 N 0.48469(13) 0.76152(8) 0.51164(15) 0.0243(4) Uani 1 1 d . . . . .
C68 C 0.43721(15) 0.77721(10) 0.44581(17) 0.0238(5) Uani 1 1 d . . . . .
N69 N 0.43639(13) 0.82688(8) 0.44841(14) 0.0243(4) Uani 1 1 d . . . . .
C70 C 0.47805(15) 0.84633(9) 0.52177(17) 0.0230(5) Uani 1 1 d . . . . .
H70 H 0.5144 0.8723 0.5032 0.028 Uiso 1 1 calc R . . . .
O71 O 0.43144(13) 0.84761(8) 0.74640(13) 0.0331(4) Uani 1 1 d . . . . .
O72 O 0.40267(11) 0.75234(7) 0.39337(13) 0.0290(4) Uani 1 1 d . . . . .
C73 C 0.53497(18) 0.76847(10) 0.71318(18) 0.0296(6) Uani 1 1 d . . . . .
H73A H 0.5307 0.7824 0.7728 0.036 Uiso 1 1 calc R . . . .
H73B H 0.5900 0.7634 0.7009 0.036 Uiso 1 1 calc R . . . .
C74 C 0.52167(18) 0.71444(10) 0.50439(18) 0.0291(6) Uani 1 1 d . . . . .
H74A H 0.5111 0.7009 0.4455 0.035 Uiso 1 1 calc R . . . .
H74B H 0.5777 0.7187 0.5098 0.035 Uiso 1 1 calc R . . . .
N75 N 0.49660(15) 0.72185(9) 0.71237(16) 0.0298(5) Uani 1 1 d . . . . .
C76 C 0.44933(16) 0.70798(10) 0.77977(17) 0.0272(5) Uani 1 1 d . . . . .
N77 N 0.43544(15) 0.65910(9) 0.77152(15) 0.0289(5) Uani 1 1 d . . . . .
C78 C 0.47847(19) 0.63733(10) 0.70056(18) 0.0316(6) Uani 1 1 d . . . . .
H78 H 0.5145 0.6120 0.7225 0.038 Uiso 1 1 calc R . . . .
N79 N 0.4325(2) 0.61996(10) 0.62838(17) 0.0434(7) Uani 1 1 d . . . . .
C80 C 0.4441(2) 0.64570(11) 0.5527(2) 0.0371(7) Uani 1 1 d . . . . .
N81 N 0.49624(16) 0.68072(9) 0.57008(15) 0.0308(5) Uani 1 1 d . . . . .
C82 C 0.52228(18) 0.68122(10) 0.66019(19) 0.0302(6) Uani 1 1 d . . . . .
H82 H 0.5790 0.6769 0.6641 0.036 Uiso 1 1 calc R . . . .
O83 O 0.42518(12) 0.73358(7) 0.83848(13) 0.0295(4) Uani 1 1 d . . . . .
O84 O 0.41408(19) 0.63783(11) 0.48141(16) 0.0562(8) Uani 1 1 d . . . . .
C85 C 0.38999(18) 0.63335(11) 0.83515(18) 0.0297(6) Uani 1 1 d . . . . .
H85A H 0.3865 0.6531 0.8892 0.036 Uiso 1 1 calc R . . . .
H85B H 0.4167 0.6030 0.8505 0.036 Uiso 1 1 calc R . . . .
C86 C 0.3899(2) 0.57544(11) 0.6302(2) 0.0414(8) Uani 1 1 d . . . . .
H86A H 0.4177 0.5518 0.6671 0.050 Uiso 1 1 calc R . . . .
H86B H 0.3871 0.5622 0.5699 0.050 Uiso 1 1 calc R . . . .
N87 N 0.31356(16) 0.62171(9) 0.80629(16) 0.0309(5) Uani 1 1 d . . . . .
C88 C 0.2500 0.64412(14) 0.8401(3) 0.0288(8) Uani 1 2 d S T P . .
C92 C 0.2500 0.57901(14) 0.6115(3) 0.0357(10) Uani 1 2 d S T P . .
N93 N 0.31341(18) 0.58128(10) 0.66406(17) 0.0366(6) Uani 1 1 d . . . . .
C94 C 0.29407(18) 0.57884(10) 0.75650(18) 0.0299(6) Uani 1 1 d . . . . .
H94 H 0.3151 0.5490 0.7845 0.036 Uiso 1 1 calc R . . . .
O95 O 0.2500 0.67760(10) 0.8922(2) 0.0328(6) Uani 1 2 d S T P . .
O96 O 0.2500 0.57563(12) 0.5317(2) 0.0455(9) Uani 1 2 d S T P . .
P101 P 0.2500 0.93512(4) 0.20106(8) 0.0520(4) Uani 1 2 d S T P . .
F102 F 0.2500 0.95952(14) 0.2958(2) 0.0717(11) Uani 1 2 d S T P . .
F103 F 0.31379(18) 0.89831(9) 0.23203(18) 0.0644(7) Uani 1 1 d . . . . .
F104 F 0.2500 0.91006(19) 0.1067(2) 0.0862(14) Uani 1 2 d S T P . .
F105 F 0.3136(2) 0.97213(11) 0.1703(2) 0.0902(11) Uani 1 1 d . . . . .
P111 P 0.5000 1.0000 0.38723(7) 0.0279(2) Uani 1 2 d S T P . .
F112 F 0.4979(2) 0.95977(12) 0.3115(2) 0.0841(10) Uani 1 1 d . . . . .
F113 F 0.40974(12) 1.00337(9) 0.3870(2) 0.0628(7) Uani 1 1 d . . . . .
F114 F 0.50257(18) 1.04153(12) 0.4563(3) 0.0887(11) Uani 1 1 d . . . . .
O201 O 0.3019(3) 0.73286(19) 0.0447(3) 0.0421(10) Uani 0.5 1 d . . . B -1
H20C H 0.2736 0.7495 0.0806 0.063 Uiso 0.5 1 d DG . . B -1
H20D H 0.2762 0.7268 -0.0028 0.063 Uiso 0.5 1 d G . . B -1
O211 O 0.2850(4) 0.7933(3) 0.1564(4) 0.071(2) Uani 0.5 1 d D . . C -1
H21A H 0.2667 0.7895 0.2092 0.107 Uiso 0.5 1 d G . . C -1
H21B H 0.2788 0.8239 0.1456 0.107 Uiso 0.5 1 d G . . C -1
O221 O 0.4628(7) 0.5873(5) 0.3412(8) 0.058(3) Uani 0.25 1 d . . . D 2
H22C H 0.4659 0.5908 0.3974 0.087 Uiso 0.25 1 d R . . E 2
H22D H 0.5036 0.6017 0.3171 0.087 Uiso 0.25 1 d R . . F 2
O231 O 0.3679(6) 0.5496(3) 0.4022(6) 0.046(2) Uani 0.25 1 d . . . G 1
H5A H 0.2518 0.8760 0.8746 0.055 Uiso 0.5 1 d R . . H -1
H5B H 0.3109 0.8668 0.8030 0.055 Uiso 0.5 1 d R . . I -1
H23A H 0.4042 0.5704 0.4096 0.069 Uiso 0.25 1 d R . . J 1
H23B H 0.3274 0.5568 0.4270 0.069 Uiso 0.25 1 d R . . K 1
O241 O 0.6443(10) 0.6165(8) 0.3987(10) 0.120(7) Uani 0.5 1 d . . . L -1
H24C H 0.6228 0.6269 0.3508 0.180 Uiso 0.5 1 d G . . L -1
H24D H 0.6172 0.5915 0.4138 0.180 Uiso 0.5 1 d G . . L -1
O251 O 0.6640(12) 0.6509(7) 0.5474(12) 0.096(5) Uani 0.25 1 d . . . M -1
H25A H 0.6677 0.6821 0.5528 0.145 Uiso 0.25 1 d R . . N -1
H25B H 0.6434 0.6467 0.4960 0.145 Uiso 0.25 1 d R . . O -1
O261 O 0.5754(8) 0.5649(9) 0.5362(15) 0.110(6) Uani 0.25 1 d . . . P -1
H26A H 0.5461 0.5402 0.5094 0.166 Uiso 0.25 1 d R . . Q -1
H26B H 0.6037 0.5525 0.5713 0.166 Uiso 0.25 1 d R . . R -1
O271 O 0.485(2) 0.493(2) 0.451(2) 0.096(5) Uani 0.125 1 d . . . S -1
H27A H 0.5047 0.4762 0.4082 0.145 Uiso 0.125 1 d R . . T -1
H27B H 0.4610 0.5153 0.4319 0.145 Uiso 0.125 1 d R . . U -1
O281 O 0.5562(8) 0.5504(9) 0.6033(15) 0.110(6) Uani 0.25 1 d . . . V 2
H28A H 0.5995 0.5427 0.6177 0.166 Uiso 0.25 1 d R . . W 2
H28B H 0.5303 0.5525 0.6570 0.166 Uiso 0.25 1 d R . . X 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 1 0 0.0229
-11 -1 0 0.0279
0 -18 2 0.0232
0 18 2 0.0434
0 -1 -10 0.0658
0 -1 10 0.0834
0 17 -4 0.0772
0 -17 -3 0.0456
-11 -5 -1 0.0334
0 17 3 0.0470
-7 13 -2 0.0551
-9 0 -6 0.0527
-3 17 1 0.0466
7 -7 -7 0.0598
-6 -14 2 0.0311
-7 15 1 0.0470
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2 104.8 . . ?
C1 C2 C4 114.5(9) . . ?
C3 C2 C1 112.3(8) . . ?
C3 C2 H2 104.8 . . ?
C3 C2 C4 114.4(11) . . ?
C4 C2 H2 104.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 110.0 . . ?
C2 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N5 C4 C2 108.5(9) . . ?
N5 C4 H4A 110.0 . . ?
N5 C4 H4B 110.0 . . ?
C4 N5 H5A 103.1(8) . . ?
C4 N5 H5B 111.7(8) . . ?
C6 N5 C4 109.6(7) . . ?
C6 N5 H5A 106.6(6) . . ?
C6 N5 H5B 106.8(5) . . ?
H5A N5 H5B 118.8(6) . . ?
N5 C6 H6A 108.9 . . ?
N5 C6 H6B 108.9 . . ?
N5 C6 C7 113.4(5) . . ?
H6A C6 H6B 107.7 . . ?
C7 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C6 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C6 C7 C8 114.9(9) . . ?
H7A C7 H7B 107.5 . . ?
C8 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 C7 113.9(6) . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C8 C9 C10 112.2(5) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
C9 C10 C11 112.8(5) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
C10 C11 H11A 107.2 . . ?
C10 C11 H11B 107.2 . . ?
H11A C11 H11B 106.8 . . ?
N12 C11 C10 120.6(6) . . ?
N12 C11 H11A 107.2 . . ?
N12 C11 H11B 107.2 . . ?
C11 N12 H12A 106.8 . . ?
C11 N12 H12B 106.8 . . ?
C11 N12 C13 122.1(5) . . ?
H12A N12 H12B 106.7 . . ?
C13 N12 H12A 106.8 . . ?
C13 N12 H12B 106.8 . . ?
N12 C13 H13A 106.7 . . ?
N12 C13 H13B 106.7 . . ?
N12 C13 C14 122.5(5) . . ?
H13A C13 H13B 106.6 . . ?
C14 C13 H13A 106.7 . . ?
C14 C13 H13B 106.7 . . ?
C13 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
C13 C14 C15 112.5(4) . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C14 C15 C17 99.2(4) . . ?
C14 C15 C18 105.8(4) . . ?
C16 C15 C14 120.3(4) . . ?
C16 C15 C17 112.2(5) . . ?
C16 C15 C18 116.3(5) . . ?
C18 C15 C17 99.9(4) . . ?
C15 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C15 C16 C19 112.0(6) . . ?
H16A C16 H16B 107.9 . . ?
C19 C16 H16A 109.2 . . ?
C19 C16 H16B 109.2 . . ?
C15 C17 H17A 110.1 . . ?
C15 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C21 C17 C15 108.2(9) . . ?
C21 C17 H17A 110.1 . . ?
C21 C17 H17B 110.1 . . ?
C15 C18 H18A 109.9 . . ?
C15 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
C23 C18 C15 108.9(5) . . ?
C23 C18 H18A 109.9 . . ?
C23 C18 H18B 109.9 . . ?
C16 C19 H19 110.1 . . ?
C16 C19 C20 107.1(10) . . ?
C20 C19 H19 110.1 . . ?
C24 C19 C16 109.8(6) . . ?
C24 C19 H19 110.1 . . ?
C24 C19 C20 109.7(11) . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 C19 112.2(19) . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C17 C21 H21 110.8 . . ?
C20 C21 C17 104(2) . . ?
C20 C21 H21 110.8 . . ?
C22 C21 C17 108.6(12) . . ?
C22 C21 C20 112.2(19) . . ?
C22 C21 H21 110.8 . . ?
C21 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C21 C22 C23 111.6(11) . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C18 C23 H23 110.1 . . ?
C18 C23 C24 107.7(8) . . ?
C22 C23 C18 110.3(7) . . ?
C22 C23 H23 110.1 . . ?
C22 C23 C24 108.6(7) . . ?
C24 C23 H23 110.1 . . ?
C19 C24 C23 110.5(7) . . ?
C19 C24 H24A 109.6 . . ?
C19 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
N53 C52 N53 108.1(3) . 4 ?
O59 C52 N53 125.96(15) . . ?
O59 C52 N53 125.96(15) . 4 ?
C52 N53 C54 112.9(2) . . ?
C52 N53 C61 122.6(2) . . ?
C61 N53 C54 124.2(2) . . ?
N53 C54 C54 103.07(14) . 4 ?
N53 C54 H54 111.8 . . ?
C54 C54 H54 111.8 4 . ?
N55 C54 N53 114.7(2) . . ?
N55 C54 C54 103.04(14) . 4 ?
N55 C54 H54 111.8 . . ?
C54 N55 C62 123.3(2) . . ?
C56 N55 C54 113.0(2) . . ?
C56 N55 C62 121.7(2) . . ?
N55 C56 N55 107.7(3) 4 . ?
O60 C56 N55 126.14(16) . . ?
O60 C56 N55 126.14(16) . 4 ?
N53 C61 H61A 108.9 . . ?
N53 C61 H61B 108.9 . . ?
N53 C61 N63 113.4(2) . . ?
H61A C61 H61B 107.7 . . ?
N63 C61 H61A 108.9 . . ?
N63 C61 H61B 108.9 . . ?
N55 C62 H62A 108.8 . . ?
N55 C62 H62B 108.8 . . ?
N55 C62 N69 114.0(2) . . ?
H62A C62 H62B 107.7 . . ?
N69 C62 H62A 108.8 . . ?
N69 C62 H62B 108.8 . . ?
C61 N63 C70 123.2(2) . . ?
C64 N63 C61 121.0(2) . . ?
C64 N63 C70 111.5(2) . . ?
N65 C64 N63 107.9(2) . . ?
O71 C64 N63 125.7(3) . . ?
O71 C64 N65 126.4(3) . . ?
C64 N65 C66 113.1(2) . . ?
C64 N65 C73 122.9(2) . . ?
C66 N65 C73 123.8(2) . . ?
N65 C66 H66 111.8 . . ?
N65 C66 N67 114.5(2) . . ?
N65 C66 C70 103.1(2) . . ?
N67 C66 H66 111.8 . . ?
N67 C66 C70 103.3(2) . . ?
C70 C66 H66 111.8 . . ?
C66 N67 C74 121.5(2) . . ?
C68 N67 C66 112.1(2) . . ?
C68 N67 C74 119.7(2) . . ?
N67 C68 N69 107.6(2) . . ?
O72 C68 N67 126.9(3) . . ?
O72 C68 N69 125.5(2) . . ?
C68 N69 C62 121.1(2) . . ?
C68 N69 C70 113.1(2) . . ?
C70 N69 C62 125.3(2) . . ?
N63 C70 C66 102.9(2) . . ?
N63 C70 H70 111.8 . . ?
C66 C70 H70 111.8 . . ?
N69 C70 N63 115.3(2) . . ?
N69 C70 C66 102.4(2) . . ?
N69 C70 H70 111.8 . . ?
N65 C73 H73A 108.6 . . ?
N65 C73 H73B 108.6 . . ?
N65 C73 N75 114.5(2) . . ?
H73A C73 H73B 107.6 . . ?
N75 C73 H73A 108.6 . . ?
N75 C73 H73B 108.6 . . ?
N67 C74 H74A 109.0 . . ?
N67 C74 H74B 109.0 . . ?
H74A C74 H74B 107.8 . . ?
N81 C74 N67 113.0(2) . . ?
N81 C74 H74A 109.0 . . ?
N81 C74 H74B 109.0 . . ?
C76 N75 C73 121.3(2) . . ?
C76 N75 C82 112.3(2) . . ?
C82 N75 C73 123.5(3) . . ?
N75 C76 N77 108.2(2) . . ?
O83 C76 N75 126.5(3) . . ?
O83 C76 N77 125.3(3) . . ?
C76 N77 C78 112.7(2) . . ?
C76 N77 C85 121.4(2) . . ?
C85 N77 C78 125.5(2) . . ?
N77 C78 H78 111.7 . . ?
N77 C78 C82 102.9(2) . . ?
N79 C78 N77 114.7(3) . . ?
N79 C78 H78 111.7 . . ?
N79 C78 C82 103.4(2) . . ?
C82 C78 H78 111.7 . . ?
C80 N79 C78 112.6(3) . . ?
C80 N79 C86 122.6(3) . . ?
C86 N79 C78 123.9(3) . . ?
N81 C80 N79 107.9(3) . . ?
O84 C80 N79 126.1(3) . . ?
O84 C80 N81 125.9(3) . . ?
C74 N81 C82 123.8(3) . . ?
C80 N81 C74 122.4(2) . . ?
C80 N81 C82 113.8(2) . . ?
N75 C82 C78 103.7(2) . . ?
N75 C82 H82 111.6 . . ?
C78 C82 H82 111.6 . . ?
N81 C82 N75 115.5(2) . . ?
N81 C82 C78 102.2(2) . . ?
N81 C82 H82 111.6 . . ?
N77 C85 H85A 108.6 . . ?
N77 C85 H85B 108.6 . . ?
N77 C85 N87 114.6(2) . . ?
H85A C85 H85B 107.6 . . ?
N87 C85 H85A 108.6 . . ?
N87 C85 H85B 108.6 . . ?
N79 C86 H86A 109.0 . . ?
N79 C86 H86B 109.0 . . ?
N79 C86 N93 112.9(3) . . ?
H86A C86 H86B 107.8 . . ?
N93 C86 H86A 109.0 . . ?
N93 C86 H86B 109.0 . . ?
C85 N87 C94 124.1(3) . . ?
C88 N87 C85 122.2(3) . . ?
C88 N87 C94 112.1(3) . . ?
N87 C88 N87 108.0(4) 4 . ?
O95 C88 N87 125.99(18) . 4 ?
O95 C88 N87 125.99(18) . . ?
N93 C92 N93 108.1(4) . 4 ?
O96 C92 N93 125.95(18) . 4 ?
O96 C92 N93 125.95(18) . . ?
C86 N93 C94 123.9(3) . . ?
C92 N93 C86 122.4(3) . . ?
C92 N93 C94 112.2(3) . . ?
N87 C94 C94 103.58(17) . 4 ?
N87 C94 H94 111.6 . . ?
N93 C94 N87 114.5(2) . . ?
N93 C94 C94 103.49(18) . 4 ?
N93 C94 H94 111.6 . . ?
C94 C94 H94 111.6 4 . ?
F102 P101 F104 179.3(2) . . ?
F103 P101 F102 90.23(15) 4 . ?
F103 P101 F102 90.23(15) . . ?
F103 P101 F103 89.5(2) . 4 ?
F103 P101 F104 89.29(17) 4 . ?
F103 P101 F104 89.29(17) . . ?
F103 P101 F105 90.66(18) . . ?
F103 P101 F105 179.7(2) . 4 ?
F103 P101 F105 179.7(2) 4 . ?
F103 P101 F105 90.67(18) 4 4 ?
F105 P101 F102 89.57(18) 4 . ?
F105 P101 F102 89.57(18) . . ?
F105 P101 F104 90.91(19) . . ?
F105 P101 F104 90.91(19) 4 . ?
F105 P101 F105 89.2(3) 4 . ?
F112 P111 F112 88.1(3) 2_675 . ?
F113 P111 F112 90.94(17) 2_675 2_675 ?
F113 P111 F112 88.85(17) 2_675 . ?
F113 P111 F112 90.94(17) . . ?
F113 P111 F112 88.85(17) . 2_675 ?
F113 P111 F113 179.7(2) . 2_675 ?
F114 P111 F112 88.3(2) 2_675 . ?
F114 P111 F112 176.5(2) . . ?
F114 P111 F112 176.5(2) 2_675 2_675 ?
F114 P111 F112 88.3(2) . 2_675 ?
F114 P111 F113 89.25(16) 2_675 2_675 ?
F114 P111 F113 90.95(16) . 2_675 ?
F114 P111 F113 89.25(16) . . ?
F114 P111 F113 90.95(16) 2_675 . ?
F114 P111 F114 95.2(3) 2_675 . ?
H20C O201 H20D 109.4 . . ?
H21A O211 H21B 104.3 . . ?
H22C O221 H22D 107.8(14) . . ?
H23A O231 H23B 114.2(10) . . ?
H24C O241 H24D 104.5 . . ?
H25A O251 H25B 104.5(19) . . ?
H26A O261 H26B 108(2) . . ?
H27A O271 H27B 110(4) . . ?
H28A O281 H28B 103(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.528(14) . ?
C2 H2 1.0000 . ?
C2 C3 1.432(13) . ?
C2 C4 1.597(18) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 N5 1.479(19) . ?
N5 C6 1.473(7) . ?
N5 H5A 0.884(6) . ?
N5 H5B 0.887(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.519(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.527(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.516(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.519(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.521(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 N12 1.405(6) . ?
N12 H12A 0.9100 . ?
N12 H12B 0.9100 . ?
N12 C13 1.455(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.462(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.599(6) . ?
C15 C16 1.342(7) . ?
C15 C17 1.672(8) . ?
C15 C18 1.601(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C19 1.531(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C21 1.60(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C23 1.542(9) . ?
C19 H19 1.0000 . ?
C19 C20 1.539(19) . ?
C19 C24 1.530(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.529(14) . ?
C21 H21 1.0000 . ?
C21 C22 1.49(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.533(13) . ?
C23 H23 1.0000 . ?
C23 C24 1.55(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C52 N53 1.369(3) 4 ?
C52 N53 1.369(3) . ?
C52 O59 1.216(5) . ?
N53 C54 1.452(3) . ?
N53 C61 1.444(3) . ?
C54 C54 1.558(5) 4 ?
C54 H54 1.0000 . ?
C54 N55 1.444(3) . ?
N55 C56 1.368(3) . ?
N55 C62 1.445(3) . ?
C56 N55 1.368(3) 4 ?
C56 O60 1.226(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 N63 1.459(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 N69 1.446(3) . ?
N63 C64 1.383(3) . ?
N63 C70 1.460(3) . ?
C64 N65 1.369(4) . ?
C64 O71 1.216(4) . ?
N65 C66 1.441(3) . ?
N65 C73 1.448(3) . ?
C66 H66 1.0000 . ?
C66 N67 1.451(4) . ?
C66 C70 1.556(3) . ?
N67 C68 1.372(3) . ?
N67 C74 1.461(3) . ?
C68 N69 1.378(4) . ?
C68 O72 1.216(3) . ?
N69 C70 1.439(3) . ?
C70 H70 1.0000 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 N75 1.457(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 N81 1.440(3) . ?
N75 C76 1.373(4) . ?
N75 C82 1.450(4) . ?
C76 N77 1.383(4) . ?
C76 O83 1.217(4) . ?
N77 C78 1.448(4) . ?
N77 C85 1.442(4) . ?
C78 H78 1.0000 . ?
C78 N79 1.444(4) . ?
C78 C82 1.564(4) . ?
N79 C80 1.370(4) . ?
N79 C86 1.442(4) . ?
C80 N81 1.358(4) . ?
C80 O84 1.226(4) . ?
N81 C82 1.446(4) . ?
C82 H82 1.0000 . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C85 N87 1.443(4) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
C86 N93 1.443(5) . ?
N87 C88 1.373(4) . ?
N87 C94 1.451(4) . ?
C88 N87 1.373(4) 4 ?
C88 O95 1.221(5) . ?
C92 N93 1.369(4) 4 ?
C92 N93 1.369(4) . ?
C92 O96 1.218(6) . ?
N93 C94 1.449(4) . ?
C94 C94 1.541(6) 4 ?
C94 H94 1.0000 . ?
P101 F102 1.593(4) . ?
P101 F103 1.584(3) 4 ?
P101 F103 1.584(3) . ?
P101 F104 1.596(4) . ?
P101 F105 1.584(3) 4 ?
P101 F105 1.584(3) . ?
P111 F112 1.605(3) . ?
P111 F112 1.605(3) 2_675 ?
P111 F113 1.580(2) . ?
P111 F113 1.580(2) 2_675 ?
P111 F114 1.561(2) 2_675 ?
P111 F114 1.561(2) . ?
O201 H20C 0.8703 . ?
O201 H20D 0.8685 . ?
O211 H21A 0.8716 . ?
O211 H21B 0.8695 . ?
O221 H22C 0.863(12) . ?
O221 H22D 0.896(13) . ?
O231 H23A 0.864(10) . ?
O231 H23B 0.827(11) . ?
O241 H24C 0.8698 . ?
O241 H24D 0.8703 . ?
O251 H25A 0.87(2) . ?
O251 H25B 0.87(2) . ?
O261 H26A 0.95(3) . ?
O261 H26B 0.806(16) . ?
O271 H27A 0.86(4) . ?
O271 H27B 0.81(5) . ?
O281 H28A 0.817(15) . ?
O281 H28B 0.94(2) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
11.3276 0.9437 0.0317 -0.0248 -0.9976 -0.0648
-11.3276 -0.9437 -0.0317 0.0248 0.9976 0.0648
-0.0234 -17.5117 2.2882 0.5383 -0.0160 0.8426
0.1126 17.5394 2.2267 -0.1075 0.0057 -0.9942
-0.1999 -1.4261 -9.8545 -0.9152 0.0217 0.4024
0.1923 -0.6335 9.8792 0.9552 -0.0231 -0.2952
-0.0083 16.6697 -3.7298 -0.6606 0.0188 -0.7505
-0.1292 -17.0554 -3.1639 0.0092 -0.0032 1.0000
-10.9899 -4.9607 -0.9991 0.0054 0.9645 0.3073
0.0097 16.9902 2.9971 -0.0238 0.0138 -0.9908
-6.9846 12.5123 -2.4979 -0.4605 0.6291 -0.5646
-8.9895 0.0251 -5.9947 -0.5647 0.7957 0.2092
-2.9867 16.9986 0.9989 -0.2120 0.2790 -0.9211
6.9880 -6.5246 -7.4931 -0.6033 -0.6180 0.5824
-6.0012 -14.4677 2.4979 0.5083 0.5137 0.6835
-6.9835 14.5141 1.4984 -0.1152 0.6286 -0.8023
